CN104511290A - Preparation method of visible-light-driven photocatalyst nano spherical MoSe2 material - Google Patents
Preparation method of visible-light-driven photocatalyst nano spherical MoSe2 material Download PDFInfo
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- CN104511290A CN104511290A CN201410853064.6A CN201410853064A CN104511290A CN 104511290 A CN104511290 A CN 104511290A CN 201410853064 A CN201410853064 A CN 201410853064A CN 104511290 A CN104511290 A CN 104511290A
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Abstract
The invention provides a preparation method of a visible-light-driven photocatalyst nano spherical MoSe2 material. The preparation method comprises the following steps: weighing sodium molybdate and organic selenium source selenium sodium cyanoacetate, dissolving sodium molybdate in deionized water to prepare a sodium molybdate solution, dissolving the selenium sodium cyanoacetate in glycol to prepare a selenium sodium cyanoacetate solution, mixing and fully stirring the sodium molybdate solution and the selenium sodium cyanoacetate solution until the solutions are clear and uniformly mixed to prepare mixed liquor; transferring the mixed liquor to a high-pressure reaction kettle using teflon as the lining, and heating in a water bath to obtain a reaction product; centrifuging the reaction product through a centrifugal machine, collecting the lower precipitate and washing by deionized water and ethyl alcohol; drying the washed product and carrying out annealing treatment by a vacuum tube furnace in inert atmosphere to prepare the nano spherical MoSe2 material. The preparation method overcomes the defects in the prior art, and is safe and environment-friendly in the production process and particularly suitable for large-scale industrial production.
Description
Technical field
The invention provides the spherical MoSe of a kind of visible light catalytic nanometer
2the preparation method of material, and the application in photocatalysis field, belong to technical field of nano material.
Background technology
Since the 1970's, continuous aggravating circumstances pollute and energy shortage adds potential global crisis consciousness.In order to the sustainable development of human society, developing free of contamination environment remediation technology and alternative clean energy resource supply is a urgent task.In the various green earth and renewable energy source item carry out, conductor photocatalysis becomes one of the most promising technology.
And light-catalyzed reaction is applied in the practical application such as environmental protection and clean energy resource, the task of a core is the most exactly develop the catalysis material that solar energy utilization ratio is high under natural daylight.In the past few decades, the metal oxide that what scientific research was too much focus on based on metallic element, and seldom considered for the research potential of metal selenide.And transiens metal chalcogenide (comprises MSx and MSe
x, M represents transiens metallic element) and there are various physical property and chemical property, physical property is as semiconductive, and superconductivity, metallicity, magnetic etc., chemical property is as photocatalytic.Therefore, to prepare and the performance of studying this kind of material becomes the focus of recent research gradually.
MoSe
2be the one of magnesium-yttrium-transition metal selenides, it is a kind of novel nano-material risen recent years, and its semiconductive can be applicable to photoelectricity and photoelectron aspect.It has layer structure, is combined between Mo atom with Se atom with stronger covalent bond effect, then relies on more weak Van der Waals force to connect between layers.In addition, MoSe
2nano material is in different types of catalysis, and lubricant, there is application frictional behaviour aspect, and can effectively promote that solar energy converts electric energy to.
But MoSe
2all the starting stage is in synthetic method or application aspect.See with regard to current synthetic method, mainly there is following problem: in experimentation, 1. generally use simple substance selenium powder for selenium source, during for two phase reaction, can not contact very well, and reaction can not effectively be carried out; 2. H is adopted in experimentation
2or hydrazine hydrate is reducing agent, there is certain risk, and Product yields is low, and purity is low, and size range is wide.Therefore, new magnesium-yttrium-transition metal MoSe is started
2preparation method, overcoming now methodical shortcoming becomes the focus of current research.
Summary of the invention
The invention provides the spherical MoSe of a kind of visible light catalyst nanometer
2the preparation method of material, solves the deficiency in background technology, and its production process safety and environmental protection, is particularly suitable for large-scale industrial production.
Realizing the technical scheme that above-mentioned purpose of the present invention adopts is:
The spherical MoSe of a kind of visible light catalyst nanometer
2the preparation method of material, comprises the following steps:
(1), sodium molybdate and organic selenium source selenium cyanoacetic acid sodium is taken according to the mol ratio of 1:2 ~ 3, sodium molybdate being dissolved in obtained concentration in deionized water is the sodium molybdate solution of 0.8 ~ 1.4moL/L, selenium cyanoacetic acid sodium being dissolved in obtained concentration in ethylene glycol is the selenium cyanoacetic acid sodium solution of 1.6 ~ 4.2moL/L, sodium molybdate solution and selenium cyanoacetic acid sodium solution are carried out mixing and fully stirs, until solution clarification also fully mixes, obtained mixed liquor;
(2), by mixed liquor being transferred to liner is in the autoclave of polytetrafluoroethylene (PTFE), at the Water Under bath heating 24 ~ 72h of 180 DEG C ~ 210 DEG C, obtains product;
(3), by product by centrifuge, collect lower sediment thing, and wash with deionized water, ethanol;
(4), wash after product dry, recycling vacuum tube furnace annealing in process under inert atmosphere, the condition of 300 ~ 550 DEG C, can obtain the spherical MoSe of visible light catalyst nanometer
2material.
Inert atmosphere described in step (4) is argon gas or nitrogen.
By spherical for nanometer MoSe in the present invention
2the concentration that material joins 100mL is in the rhodamine B solution of 20ppm, and under then mixture solution being placed in dark condition, dark treatment magnetic stirs 1h, makes it reach adsorption equilibrium, then adds 5 ~ 10mL H
2o
2, or do not add.Under wavelength is greater than the filter plate of light can being irradiated of 420nm, finally carry out the light-catalyzed reaction of visible ray.Take out 10mL suspended sample every 10min in course of reaction, be then separated by centrifuge, and the supernatant liquor obtained is surveyed its corresponding absorbance by ultraviolet specrophotometer.After tested, under visible light illumination, hydrogen peroxide exists in system and presents excellent photocatalysis performance.
Compared with prior art, the present invention utilizes simple hydrothermal reaction at low temperature to prepare MoSe
2nanoparticle, production process safety and environmental protection, is particularly suitable for large-scale industrial production.In addition, the visible light catalyst MoSe utilizing the method to prepare
2the degree of crystallinity that nanoparticle has had, purity is high.
Accompanying drawing explanation
The spherical MoSe of nanometer that Fig. 1 provides for the embodiment of the present invention
2the XRD figure of material;
The spherical MoSe of nanometer that Fig. 2 provides for the embodiment of the present invention
2sEM figure and the TEM figure of material;
The spherical MoSe of nanometer that Fig. 3 provides for the embodiment of the present invention
2the photocatalysis performance curve map of material.
Detailed description of the invention
Below in conjunction with accompanying drawing, detailed specific description is done to the present invention, but protection scope of the present invention is not limited to following examples.
Embodiment 1
The spherical MoSe of visible light catalyst nanometer provided in the present embodiment
2the preparation method of material is as follows: by 0.02mol Na
2moO
4be dispersed in 25mL water, stir continuously and form clear solution, by organic selenium source of 0.04mol-selenium cyanoacetic acid sodium is dissolved in the ethylene glycol of 25mL in another beaker; Under room temperature, the two is mixed, mixed liquor is carried out magnetic and stir 30min, make it mix, be then transferred in 100mL autoclave, under 210 DEG C of conditions, react 24h; The product that obtains after reaction, by centrifuge centrifugal 5min under the centrifugation rate of 7000rpm, is outwelled upper solution, the lower sediment thing water obtained, ethanol are washed till few 3 times; Wash after product vacuum dried overnight, recycling vacuum tube furnace annealing in process 10h under Ar atmosphere, the condition of 450 DEG C, can obtain the spherical MoSe of visible light catalyst nanometer
2material.
Accompanying drawing 1 is the X-ray diffraction of the present embodiment product after 210 DEG C of hydrothermal treatment consists 24h (XRD) figure, and product is the good MoSe of crystallinity as seen from the figure
2, and there are not other impurity phases.
Accompanying drawing 2 is ESEM (SEM) and projection Electronic Speculum (TEM) picture of the present embodiment product, MoSe prepared as seen from the figure
2in spherical, these balls are polymerized by irregular nanoscale lamella, and prepared MoSe
2size uniformity, to be evenly distributed.
Test photochemical catalyst MoSe prepared in the present embodiment below
2the catalytic performance of nanoparticle.
By the MoSe of 50mg in the present embodiment
2the concentration that photochemical catalyst joins 100mL is in the rhodamine B solution of 20ppm, carries out magnetic and stirs 1h, make it reach adsorption equilibrium, then add 5mL H under then mixture solution being placed in dark condition
2o
2under wavelength is greater than the filter plate of light can being irradiated of 420nm, finally carry out the light-catalyzed reaction of visible ray.10mL suspended sample is taken out every 10min clock in course of reaction, then by centrifuge centrifugal 5min under the centrifugation rate of 3000rpm, by centrifugal for suspension to centrifuge tube, and the supernatant liquor obtained is surveyed its corresponding absorbance by ultraviolet specrophotometer.Not add photochemical catalyst in embodiment, other steps are identical to be tested as a comparison.
From Lamber-Beer law, the concentration of rhodamine B solution and it is proportional in the power of the absorbance of characteristic absorption wavelength, therefore, we can carry out quantitative analysis by the change of the absorbance detecting solution in photocatalytic process to rate of photocatalytic oxidation, and then weigh photochemical catalyst MoSe with degradation rate (R)
2photocatalysis effect.
R＝[(A
0-A)/A
0]×100％
A in formula
0for the absorbance before illumination; The absorbance of A to be light application time be t.
Nano-photocatalyst material MoSe
2the degradation results of catalysis rhodamine B as shown in Figure 3, can be found out, although only having MoSe
2time, under visible light conditions, rhodamine B is degraded hardly; Do not adding photochemical catalyst MoSe
2only add 5mLH
2o
2time, under visible light conditions, rhodamine B is not almost degraded.And 5mLH is added in reaction system
2o
2after, in short 40min, the degradation rate of rhodamine B reaches more than 90%.As can be seen here, the present invention is at H
2o
2under existent condition, MoSe under visible ray effect
2present good catalytic performance.This is MoSe
2good basis has been established in catalysis under visible light conditions.
Embodiment 2
The spherical MoSe of visible light catalyst nanometer provided in the present embodiment
2the preparation method of material is as follows: by 0.03molNa
2moO
4be dispersed in 25mL water, stir continuously and form clear solution, by organic selenium source of 0.09mol-selenium cyanoacetic acid sodium is dissolved in the ethylene glycol of 25mL in another beaker; Under room temperature, the two is mixed, mixed liquor is carried out magnetic and stir 30min, make it mix, be then transferred in 100mL autoclave, under 180 DEG C of conditions, react 65h; The product that obtains after reaction, by centrifuge centrifugal 5min under the centrifugation rate of 7000rpm, is outwelled upper solution, the lower sediment thing water obtained, ethanol are washed till few 3 times; Wash after product vacuum dried overnight, recycling vacuum tube furnace annealing in process 12h under Ar atmosphere, the condition of 350 DEG C, can obtain the spherical MoSe of visible light catalyst nanometer
2material.
Claims (2)
1. the spherical MoSe of visible light catalyst nanometer
2the preparation method of material, is characterized in that comprising the following steps:
(1), sodium molybdate and organic selenium source selenium cyanoacetic acid sodium is taken according to the mol ratio of 1:2 ~ 3, sodium molybdate being dissolved in obtained concentration in deionized water is 0.8 ~ 1.4moL/L sodium molybdate solution, selenium cyanoacetic acid sodium being dissolved in obtained concentration in ethylene glycol is 1.6 ~ 4.2moL/L selenium cyanoacetic acid sodium solution, sodium molybdate solution and selenium cyanoacetic acid sodium solution are carried out mixing and fully stirs, until solution clarification also fully mixes, obtained mixed liquor;
(2), by mixed liquor being transferred to liner is in the autoclave of polytetrafluoroethylene (PTFE), at the Water Under bath heating 24 ~ 72h of 180 DEG C ~ 210 DEG C, obtains product;
(3), by product by centrifuge, collect lower sediment thing, and wash with deionized water, ethanol;
(4), wash after product dry, recycling vacuum tube furnace annealing in process under inert atmosphere, the condition of 300 ~ 550 DEG C, can obtain the spherical MoSe of visible light catalyst nanometer
2material.
2. the spherical MoSe of visible light catalyst nanometer according to claim 1
2the preparation method of material, is characterized in that: the inert atmosphere described in step (4) is argon gas or nitrogen.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105271136A (en) * | 2015-10-28 | 2016-01-27 | 常州轻工职业技术学院 | Preparation method of ultra-thin nanometer hollow sphere MoSe2 |
| US20180282236A1 (en) * | 2016-01-13 | 2018-10-04 | Wuhan Sunen-Tech Co., Ltd. | Selenium-enriching enhancer for plant cultivation and preparation and use thereof |
| CN109970034A (en) * | 2019-04-29 | 2019-07-05 | 四川大学锦城学院 | A kind of ultrathin nanometer hollow sphere MoSe2The preparation method of material |
| CN111167521A (en) * | 2020-01-18 | 2020-05-19 | 河南师范大学 | Catalytic material, preparation method thereof, photocatalyst and electrocatalyst |
| CN112250044A (en) * | 2020-10-16 | 2021-01-22 | 南开大学 | Preparation method of molybdenum diselenide submicron spheres |
| CN114904011A (en) * | 2021-07-06 | 2022-08-16 | 中国科学院上海硅酸盐研究所 | Non-iron-based glutathione consumption synergistic active oxygen species reinforced composite material and preparation method and application thereof |
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| JPH0857319A (en) * | 1994-08-24 | 1996-03-05 | Mitsubishi Chem Corp | Method for activating metal oxide catalyst |
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| JPH0857319A (en) * | 1994-08-24 | 1996-03-05 | Mitsubishi Chem Corp | Method for activating metal oxide catalyst |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105271136A (en) * | 2015-10-28 | 2016-01-27 | 常州轻工职业技术学院 | Preparation method of ultra-thin nanometer hollow sphere MoSe2 |
| CN105271136B (en) * | 2015-10-28 | 2017-08-25 | 常州轻工职业技术学院 | A kind of ultrathin nanometer hollow ball MoSe2Preparation method |
| US20180282236A1 (en) * | 2016-01-13 | 2018-10-04 | Wuhan Sunen-Tech Co., Ltd. | Selenium-enriching enhancer for plant cultivation and preparation and use thereof |
| US10815158B2 (en) * | 2016-01-13 | 2020-10-27 | Wuhan Sunen-Tech Co., Ltd. | Selenium-enriching enhancer for plant cultivation and preparation and use thereof |
| CN109970034A (en) * | 2019-04-29 | 2019-07-05 | 四川大学锦城学院 | A kind of ultrathin nanometer hollow sphere MoSe2The preparation method of material |
| CN111167521A (en) * | 2020-01-18 | 2020-05-19 | 河南师范大学 | Catalytic material, preparation method thereof, photocatalyst and electrocatalyst |
| CN111167521B (en) * | 2020-01-18 | 2023-02-17 | 河南师范大学 | Catalytic material, preparation method thereof, photocatalyst and electrocatalyst |
| CN112250044A (en) * | 2020-10-16 | 2021-01-22 | 南开大学 | Preparation method of molybdenum diselenide submicron spheres |
| CN114904011A (en) * | 2021-07-06 | 2022-08-16 | 中国科学院上海硅酸盐研究所 | Non-iron-based glutathione consumption synergistic active oxygen species reinforced composite material and preparation method and application thereof |
| CN114904011B (en) * | 2021-07-06 | 2023-10-13 | 中国科学院上海硅酸盐研究所 | Non-iron-based glutathione consumption synergistic active oxygen species reinforced composite material, and preparation method and application thereof |
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